تفاعل #1842895

ord-dfc53ec76dbe4ccfbc510d42dfa32112

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas slowly added
  2. 2
    أخرىreaction
  3. 3
    workup.STIRRINGThe reaction mixture was stirred at 10° C. or below for 1 h
  4. 4
    استخلاصThen, the reaction product was extracted with dichloromethane
  5. 5
    غسيلthe extracted layer was washed with water
  6. 6
    تجفيفFurther, the extracted layer was dried over anhydrous sodium sulfate
  7. 7
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  8. 8
    أخرىThe residue was recrystallized with benzene

الإجراء التجريبي

To an ice-cooled solution of 2-methyl-l-naphthol (7.9 g, 0.05 mmol) in dichloromethane, anhydrous aluminum chloride (7.2 g) was slowly added with stirring, followed by slow addition of acetyl chloride (4.7 g) to start reaction. The reaction mixture was stirred at 10° C. or below for 1 h, then at room temperature for 3 h. Thereafter, the mixture was poured into ice water. Then, the reaction product was extracted with dichloromethane and the extracted layer was washed with water. Further, the extracted layer was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was recrystallized with benzene, giving the desired compound, 2-methyl-4-acetyl-1-naphthol, in an amount of 3.9 g .

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05438139uspto-grants-1995_08